Dimethyl Sulfate → HCID 86759321, compound

Participants

Reaction Conditions

Reaction Steps

A solution of 129.0 g of pentane-2,3,4-trione 3-oxime in 385 g of MTBE and 138.7 g of dimethyl sulfate (DMS) were added dropwise to a suspension of 165 g of potassium carbonate in a mixture of 100 g of dimethylformamide (DMF) and 300 g of tert-butyl methyl ether (MTBE) at about 20° C. with cooling. After stirring at about 20° C. for 2 h, 21.9 g of diethylamine were added to destroy excess DMS and, after stirring at about 20° C. for a further hour, 800 ml of water were added. The solution was extracted with tert-butyl methyl ether. From the combined organic phases there were obtained after washing with 1 N H2SO4 144.6 g of pentane-2,3,4-trione 3-O-methyloxime (96.5% pure according to GC analysis), corresponding to a yield of 97.6% of theory.

Provenance & Evidence